Agilent Technologies 7697A Installation And Startup Manual

Agilent Technologies

Agilent 7697A

Headspace Sampler

Installation and First Startup

Notices

No part of this manual may be reproduced

in any form or by any means (including

electronic storage and retrieval or

translation into a foreign language) without

prior agreement and written consent from

Agilent Technologies, Inc. as governed by

United States and international copyright

laws.

Manual Part Number

G4556-90013

Edition

Fourth edition, May 2012

Third edition, February 2012

Second edition, November 2011

First edition, January 2011

Printed in USA

Agilent Technologies, Inc.

2850 Centerville Road 

Wilmington, DE 19808-1610 USA

安捷伦科技（上海）有限公司

上海市浦东新区外高桥保税区

英伦路 412 号

联系电话：（800）820 3278

Warranty

The material contained in this document

is provided “as is,” and is subject to being

changed, without notice, in future

editions. Further, to the maximum extent

permitted by applicable law, Agilent

disclaims all warranties, either express

or implied, with regard to this manual and

any information contained herein,

including but not limited to the implied

warranties of merchantability and fitness

for a particular purpose. Agilent shall not

be liable for errors or for incidental or

consequential damages in connection

with the furnishing, use, or performance

of this document or of any information

contained herein. Should Agilent and the

user have a separate written agreement

with warranty terms covering the

material in this document that conflict

with these terms, the warranty terms in

the separate agreement shall control.

Safety Notices

CAUTION

A CAUTION notice denotes a hazard. It

calls attention to an operating

procedure, practice, or the like that, if

not correctly performed or adhered to,

could result in damage to the product

or loss of important data. Do not

proceed beyond a CAUTION notice

until the indicated conditions are fully

understood and met.

WARNING

A WARNING notice denotes a hazard.

It calls attention to an operating

procedure, practice, or the like that, if

not correctly performed or adhered to,

could result in personal injury or

death. Do not proceed beyond a

WARNING notice until the indicated

conditions are fully understood and

met.

Installation and First Startup 3

Contents

1 Installation

Before You Begin 6

Tools required for installation 6

Personnel needed for installation 6

Parts supplied with the instrument 7

Verify site preparation 8

Prepare the GC and data system 8

Determine how you will connect the headspace sampler to the GC 9

Install the GC consumables needed for HS checkout 13

Inspecting the Headspace Sampler 14

Place the Headspace Sampler on the Bench 15

Install the Configuration Plug 17

Verify the available power configuration 17

Install the configuration plug 18

Install the Vial Tray (111 Vial Model Only) 21

Connect Cabling 26

Cabling diagrams for Agilent GCs 27

Other systems 28

Connect Gas Supplies 30

Connect the vial pressurization gas 31

Connect the carrier gas (using GC inlet carrier control) 32

Connect the Transfer Line to the GC 35

Install the transfer line to the Headspace 36

Attach the transfer line to a GC inlet 45

Install the transfer line support bracket 47

Turn On the Headspace Sampler 49

Set the IP Address 50

To set the LAN address at the keyboard 50

To use a DHCP server 50

Configure the Headspace Sampler 51

4Installation and First Startup

2 First Startup

Tools and Materials Required 54

Load the Checkout Method in the HS 55

Make the First Connection 57

Set the Checkout Method Parameters 58

If using an Agilent data system 58

Checkout method GC parameters 58

Prepare the Checkout Sample 61

Run the Checkout Sample 62

Compare Results 64

Prepare for Your Method (Optional) 67

A Making Swagelok Connections

Making Swagelok Connections 70

Using a Swagelok Tee 73

5

Agilent 7697A Headspace Sampler

Installation and First Startup

Agilent Technologies

1

Installation

Before You Begin 6

Inspecting the Headspace Sampler 14

Place the Headspace Sampler on the Bench 15

Install the Configuration Plug 17

Install the Vial Tray (111 Vial Model Only) 21

Connect Cabling 26

Connect Gas Supplies 30

Connect the Transfer Line to the GC 35

Turn On the Headspace Sampler 49

Set the IP Address 50

Configure the Headspace Sampler 51

This guide describes how to install the Agilent 7697A

Headspace Sampler (HS). This guide assumes that the GC is

installed, configured, and operating properly, along with any

associated data system.

This chapter describes the installation steps to unpack and

install the instrument. The next chapter describes how to

start up the HS for the first time and verify it is operating

properly.

6Installation and First Startup

1Installation

Before You Begin

Before installing the headspace sampler (HS), review the

information below.

Tools required for installation

The following tools and parts are needed for installation.

The other necessary parts and tools are supplied with the

new instrument.

Personnel needed for installation

The instrument is heavy. When lifting or moving the

instrument, two persons are required.

Table 1 Tools and parts for installation

Tool Agilent part number Use

Required

Torx T-20 driver 5182-3465 Transfer line installation

Open-end wrenches:

•7/16-inch (2)

•5/16-inch

8710-0972

8710-0510

Swagelok fittings for gas connections, sample loop,

and transfer line

Tubing cutter 8710-1709 Cut 1/8-inch gas supply plumbing

Precision tubing cutter 5190-1442 Cut 1/16-inch stainless steel tubing

Included

1/4-in. x 3/16-in. wrench 8710-2618 Transfer line installation

Column cutting wafer 5181-7487 Transfer line installation

Installation 1

Installation and First Startup 7

Parts supplied with the instrument

The headspace sampler ships with consumables and

hardware sufficient for typical installation and checkout. See

Table 2 below.

Table 2 Parts supplied with the headspace sampler

Description Part number Quantity Use

Wrench, open end 3/16-in. x 1/4-in. 8710-2618 1 Transfer line connection.

LAN cable 8121-0940 1 Communications.

Cable, APG remote, 9M/9M G1530-60930 1 Communications.

Flat bottom headspace vials, 20 mL, 100/pk 5182-0837 1 Checkout.

Crimp cap, headspace, Al, PTFE/Si septum,

20 mm, 100/pk

5183-4477 Checkout.

Ergonomic manual crimper for 20 mm caps 5040-4669 Checkout.

Leak Test Kit G4556-67010 1

Vial Pressurization Connection Kit

Tubing, post-drawn, 1650 mm 1530-2239 1 Connect HS Vial Pressure fitting to the gas

supply.

Nut, stainless steel, for 1/16-in. tubing 0100-0053 1 Connect the 1/16-in. end of the post-drawn

tubing to the HS Vial Pressure fitting.

Ferrule set, stainless steel, for 1/16-in. tubing 0100-1490 1

Nut and ferrule set, 1/8-in. Swagelok,

stainless steel

5181-7482 1 Connect the 1/8-in. end of the tubing to the

gas supply.

Transfer Line Connection Kit

Fused silica, deactivated, .530 mm id x 5 m

long

160-2535-5 1 Transfer line.

Fitting, internal reducer, 1/16-in. to 1/32-in. 0100-2594 1 Transfer line connection.

Ferrule, polyamide graphite 1/32-in. 0100-2595 1 Transfer line connection.

Transfer line support assembly G3504-60620 1 Support transfer line at GC inlet. Consists of

bracket, clamp, and knurled thumbscrew.

Tubing, post-drawn, 1650 mm 1530-2239 1 Connect HS Carrier fitting to the gas supply

from the GC inlet flow module.

Union SS 1/16-inch tubing 0100-0124 1 Connect the 1/16-in. end of the post-drawn

tubing to the open end of the GC inlet carrier

line.

Column cutting wafer 5181-7487 1 Trim fused silica transfer line.

8Installation and First Startup

1Installation

Verify site preparation

Verify that the site has been prepared according to the site

preparation manual. Sufficient bench space, power supply

receptacles, supplies, gases, traps, required accessories, and

so forth must be available.

Prepare the GC and data system

If not already installed, install the gas chromatograph and

verify its performance before beginning HS installation.

•Install the GC.

•Install the data system.

•Verify GC and data system performance.

•Cool all heated zones in the GC to safe handling

temperatures, especially the column oven and the inlet.

HS installation requires carrier gas flow interruption,

which can damage a hot column. HS installation requires

contact with the GC inlet, which can be hot enough to

cause burns.

•If you purchased the add- on HS control software, install

it after installing the data system.

Cap, 1/16-in., stainless steel 0100-0050 1 Cap the cut end of the SSL or MMI inlet

carrier tubing.

Nut and ferrule set, 1/8-in. Swagelok,

stainless steel

5181-7482 1 Connect the 1/8-in. end of the post-drawn

tubing to the HS.

Nut, stainless steel, for 1/16-in. tubing 0100-0053 1 Cap the cut end of the SSL or MMI inlet

carrier tubing.

Ferrule set, stainless steel, for 1/16-in. tubing 0100-1490 1

Septum retainer nut for transfer line G3452-60835 1 Support transfer line on GC SSL or MMI inlet

Liner, Direct Connect, 2 mm ID, deactivated 5181-8818 1 GC SSL or MM inlet liner for checkout.

O-Ring, 2-010, Fluoroelastomer, 10/pk 5188-5365 1 GC SSL or MM inlet liner O-ring.

Septa, 11 mm low bleed, 5/pk 5182-3413 1 GC SSL or MM inlet septum (for checkout).

Table 2 Parts supplied with the headspace sampler (continued)

Description Part number Quantity Use

Installation 1

Installation and First Startup 9

Determine how you will connect the headspace sampler to the GC

How you connect the headspace sampler to the GC depends

on:

•The GC model

•The GC inlet type

•Optional HS accessories

•Whether or not you need to also use this same GC inlet

for other injection types (ALS or manual, for example)

See Table 3. Determine the connection best suited to your

hardware and needs.

Table 3 Supported headspace sampler–GC connections and control modes

Inlet type GC models Connection type Supports HS

carrier mode(s)

Comments

Recommended configurations

Split/

splitless,

Multimode

7890, 7820,

6890, 6850,

5975T

Transfer line through

septum head

•GC controls

carrier flow

•GC + HS

(additive)*

•Standard configuration.

•Can be disconnected to support

autosampler or manual injection.

•With GC control of carrier flow, HS must be

On for non-HS injections.

•Supports frequent column changes.

Optional hardware:

•G4562A Carrier Gas EPC Module

Accessory.

•G3521A 7890A S/SL MMI Weldment for

Headspace (7890A, 5975T only).

* Requires G4562A Carrier Gas EPC Module Accessory

10 Installation and First Startup

1Installation

Split/

splitless,

Multimode

7890 G3520A Transfer Line

Interface Accessory

GC controls carrier

flow

•Allows alternating HS and ALS usage,

without hardware changes.

•Transfer line bypasses septum, reducing

cross-contamination between runs.

•Design reduces cold spots, improves

performance for samples with analytes

such as high weight alkenes (C40).

•Best performance for widest range of

analyses.

•Supports frequent column changes.

•Reduces potential for leaks.

•With GC control of carrier flow, HS must be

On for non-HS injections.

Required hardware:

•G3520A Transfer Line Interface Accessory.

•1/16-inch stainless steel tubing.

Optional hardware:

•G4562A Carrier Gas EPC Module

Accessory.

Volatiles

interface

7890, 6890 Transfer line direct to

volatiles interface

GC controls carrier

flow

•No support for additive flow.

•High sensitivity.

•Allows small volume injections.

•Most inert choice.

•Not recommended for frequent column

changes.

•Does not support ALS or manual injections.

Required hardware:

•Strain relief adapter.

Optional configurations

Split/

splitless,

Multimode

7890, 7820,

6890, 6850,

5975T

Transfer line through

septum head

•HS controls

carrier flow*

•GC + HS

(additive)*

•Can be disconnected to support

autosampler or manual injection.

•Carrier flow control not as robust as control

available using GC.

Required hardware:

•G4562A Carrier Gas EPC Module

Accessory.

Table 3 Supported headspace sampler–GC connections and control modes (continued)

Inlet type GC models Connection type Supports HS

carrier mode(s)

Comments

* Requires G4562A Carrier Gas EPC Module Accessory

Installation 1

Installation and First Startup 11

Purged

packed

7890, 7820,

6890, 6850

Transfer line through

septum head

GC + HS (additive)* Purged packed inlet is not recommended for

HS use. The flow rate through the transfer line

needs to be high, which broadens peaks. If

used, set only a small flow from the PP inlet

(to sweep the inlet septum). Provide the main

column flow using the HS additive flow.

•Supports frequent column changes.

•Can be disconnected to support

autosampler or manual injection.

•Users will need to experiment with flows to

optimize the analysis.

Required hardware:

•G4562A Carrier Gas EPC Module

Accessory.

Cool

on-column

7890, 6890,

6850

Transfer line through

septum head

GC controls carrier

flow

Cool on-column inlet is not recommended for

HS use. For most analytes, instead use a SSL

or MMI and run the column up and through

the transfer line to the HS 6 port valve. (Use of

columns > 530 µm is not recommended in the

transfer line. Larger id columns are not

supported for this use.) If connecting the

column directly to the HS sampling valve, for

most analytes provide a small split flow so

that the inlet provides a small amount to

sweep septum, and let the HS provide most

flow, for example 0.1:1.

•The flow rate through the transfer line

needs to be high, which broadens peaks.

•Supports frequent column changes.

•Can be disconnected to support

autosampler or manual injection, but

realignment of ALS or change of inlet

hardware may be required.

•Users will need to experiment with flows to

optimize the analysis.

•With the cool on-column inlet, the transfer

line butts against column. This is not

preferred.

Required hardware:

•G4562A Carrier Gas EPC Module

Accessory.

•Cool on-column inlet hardware for transfer

line size.

Table 3 Supported headspace sampler–GC connections and control modes (continued)

Inlet type GC models Connection type Supports HS

carrier mode(s)

Comments

* Requires G4562A Carrier Gas EPC Module Accessory

12 Installation and First Startup

1Installation

Any

non-Agilent

any

non-Agilent

User must determine

connection method

•GC + HS

(additive)*

•HS controls

carrier flow

•Determine best modes and use cases

based on similar Agilent hardware.

Required hardware:

•G4562A Carrier Gas EPC Module

Accessory.

Table 3 Supported headspace sampler–GC connections and control modes (continued)

Inlet type GC models Connection type Supports HS

carrier mode(s)

Comments

* Requires G4562A Carrier Gas EPC Module Accessory

Installation 1

Installation and First Startup 13

Install the GC consumables needed for HS checkout

HS checkout requires the GC consumables listed in Table 4.

Install them before installing the HS. See your GC user

documentation for details.

Configure the column and any other items, as needed.

Table 4 GC consumables needed for HS performance verification

Description Part number

GC checkout column:

7890, 7820, 6890:

6850:

If using MS or MSD:

7890, 7820, 6890:

6850:

5975T:

19091J-413

19091J-413E

19091S-433

19091S-433E

G3900-63001

Helium carrier gas

For split/splitless or multimode inlet

Liner 5181-8818*

Liner O-ring 5188-6405*

If using FID or NPD

Makeup gas Nitrogen or helium

If using µECD

Makeup gas Nitrogen or argon/methane

*Supplied with the HS.

14 Installation and First Startup

1Installation

Inspecting the Headspace Sampler

Inspect the headspace sampler (HS) shipping container(s).

1Inspect the shipping containers for damage. If a container

is damaged or shows signs of stress, notify both the

carrier and your local Agilent office.

Keep all shipping materials for inspection by the carrier.

2Check the items received against the packing lists. If there

are discrepancies, notify your local Agilent office

immediately.

Keep the shipping containers until you have checked their

contents for completeness and verified instrument

performance.

WARNING

The instrument is heavy. Use extreme caution when handling the

instrument. A two person lift is recommended. Failure to perform a

two person lift may result in personal injury.

Installation 1

Installation and First Startup 15

Place the Headspace Sampler on the Bench

The HS requires a benchtop that can support its weight plus

that of other equipment you will use with it. The area must

be free of overhanging obstructions that might interfere with

cooling and limit access to the top of the instrument.

1Remove the HS from its shipping box.

•Be careful when removing the packing foam from

around the instrument. The foam also secures the

transfer line.

2Place the HS on the benchtop. Make sure gas and power

supplies are accessible. Place other required equipment

near the HS. Install only on the right side of the GC.

3Remove caps and packing.

Protective caps cover gas input and vent fittings on the

back of the unit.

Remove any packing tape that secures the transfer line

against the instrument.

For the 12 vial model, lift the tray cover and remove any

packing material from the tray.

WARNING

The instrument is heavy. Use extreme caution when handling the

instrument. A two person lift is recommended. Failure to perform a

two person lift may result in personal injury.

16 Installation and First Startup

1Installation

4Unpack the tray, if purchased.

Check the tray for shipping tape and packing screws.

Remove them. Packing screws will be labeled with a flag

or ribbon for identification. Remove any tape or packing

screws found.

CAUTION

The tray gantry in secured only by the foam packing material. Be

careful when unpacking the tray. The gantry can move when you lift

the tray.

Installation 1

Installation and First Startup 17

Install the Configuration Plug

Before use, set the HS power configuration.

Verify the available power configuration

1Locate the configuration plug that shipped with the

headspace sampler. Compare the voltage shown on the

configuration plug label with the laboratory line voltage.

(For customers in Japan using 100 VAC, the unit is

120 VAC with an external 100 V/200 V step up

transformer.) See Table 5.

2Locate the power cord that shipped with the headspace

sampler. Verify the power cord is correct for the locale

and voltage.

Measure the power outlet voltage and verify it meets the

tolerance requirements listed in Table 6.

Table 5 Headspace sampler power configuration plugs

Part number Voltage Color

G4556-60390 120 VAC Brown

G4556-60400 200 VAC Red

G4556-60410 220 VAC Orange

G4556-60420 230 VAC Yellow

G4556-60430 240 VAC Violet

WARNING

Measuring the mains voltage can expose you to hazardous

electrical current. Only a trained technician should perform this

step.

18 Installation and First Startup

1Installation

Install the configuration plug

Install the configuration plug as follows:

Table 6 Power consumption

Product Line voltage (VAC) Frequency (Hz) Maximum

continuous

power

consumption

(VA)

Current rating

(amps)

Power outlet

current rating

111 Vial model 100*/120

single phase 

(–10% / +10%)

50/60 850 6.2 15 Amp

111 Vial model 200/220/230/240

single/split phase

(–10% / +10%)

50/60 850 3.8/3.4/3.3/3.1 10 Amp

12 Vial model 100*/120

single phase 

(–10% / +10%)

50/60 850 6.2 15 Amp

12 Vial model 200/220/230/240

single/split phase

(–10% / +10%)

50/60 850 3.8/3.4/3.3/3.1 10 Amp

* Users of 100 V power (Japan) receive the 120 V US power option with a 100 V/120 V step up transformer.

WARNING

Only an Agilent-trained technician should perform this procedure.

CAUTION

Components can be damaged by static electricity: be sure to wear

an ESD strap grounded to the GC chassis while performing this

procedure.

Installation 1

Installation and First Startup 19

1Locate the cover plate for the AC board on the lower back

right corner of the HS.

2Loosen the T- 20 Torx screw in the cover plate and rotate

the cover plate to expose the AC board.

Screw

Hole for

configuration

plug label

20 Installation and First Startup

1Installation

3Install the configuration plug into the AC board

(connector P4). See Figure 1.

Figure 1 Close up of AC board

4Rotate the cover plate until it covers the plug. Reinstall

the screw to secure in place. The power rating label can

be seen through the cover plate.

If the plate does not close, check the configuration plug.

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Agilent Technologies 7697A Installation And Startup Manual

Agilent Technologies 7697A Installation And Startup Manual

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